CN111874914B - Method for preparing 4N high-purity quartz sand by taking pegmatite quartz as raw material - Google Patents
Method for preparing 4N high-purity quartz sand by taking pegmatite quartz as raw material Download PDFInfo
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
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Abstract
The invention discloses a method for preparing 4N high-purity quartz sand by taking pegmatite quartz as a raw material, which comprises the following steps: (1) Crushing, grinding and screening pegmatite raw quartz to obtain pegmatite quartz powder; (2) After pegmatite quartz powder is mixed into ore pulp, the pH value of the ore pulp is regulated to 2-3, an anion collecting agent is added into the ore pulp, and after stirring, a cation collecting agent is added for flotation treatment; (3) Roasting pegmatite quartz concentrate for 3-7 h at 850-1000 ℃, and performing water quenching treatment on the pegmatite quartz concentrate after roasting is finished; (4) Mixing the pegmatite quartz concentrate subjected to roasting and water quenching with a leaching solution, and carrying out hot-pressing leaching treatment, wherein the hot-pressing leaching temperature is 220-250 ℃, the hot-pressing leaching time is 4-8 h, and the leaching solution is a mixed solution of a sulfuric acid solution and a hydrofluoric acid solution. The method can obtain the quartz sand with higher purity, and the preparation process flow is simple.
Description
Technical Field
The invention belongs to the technical field of processing and purifying of nonmetallic minerals, and particularly relates to a method for preparing 4N high-purity quartz sand by taking pegmatite quartz as a raw material.
Background
Quartz (quartz), chemical formula SiO 2 It is an important non-metallic mineral material, and common quartz sand is commonly used for ceramics, glass products and the like. And high purity quartz (high purity quartz), siO 2 The content is more than or equal to 99.9 percent, and the ultra-pure quartz material has excellent thermal property, optical property, electrical property and the like, so the ultra-pure quartz material is widely applied to the fields of optical fiber communication, aerospace, war industry, electronic technology and the like, and the ultra-pure quartz material becomes more and more important along with the rapid development of electronic information technology. High-purity quartz sand to SiO 2 The content is required to be high, and impurity elements (such as Fe, al, K, na and the like) are required to be reduced to a very low level.
The high-purity quartz is mainly prepared by taking natural quartz as a raw material, but the quartz is produced by ChinaThe source is deficient, and the preparation of high-purity quartz sand is seriously restricted. Pegmatite is so named because it often contains large-grained crystals, has a coarse-grained or a very-grained structure, and usually has a grain size of more than 50mm, with the maximum of the crystals being more than 10 m. Pegmatite is rich in quartz and is widely distributed in China. The pegmatite is used for replacing natural crystal to prepare the high-purity quartz sand, so that the domestic demand for the high-purity quartz sand can be effectively filled. The impurity elements in pegmatite rock are generally present in the form of gangue minerals, fluid inclusions, lattice impurities, etc., and if these impurity elements are not removed, siO is present 2 The content can not meet the use requirement, the added value of the product is low, and therefore pegmatite quartz needs to be purified to reduce gangue minerals and impurity elements in the pegmatite quartz.
The existing purification method of quartz sand adopts a purification process flow of 'cleaning and hand selection, primary roasting and water quenching, vacuum drying and fine crushing, secondary roasting and water quenching and acid leaching purification', the flow is complex, the concentrations of sulfuric acid and hydrofluoric acid serving as leaching agents are respectively 30% and 5%, and the consumption of the agents is large; there are also purification processes using "rod mill scrubbing-desliming-flotation-acid leaching-magnetic separation", but only SiO is finally obtained 2 The content of the refined quartz sand is more than or equal to 99.8 percent, and the economic benefit of the product is poor. Therefore, the method has the advantages of simple process flow, low medicament consumption and capability of preparing SiO 2 The production method of the high-purity quartz sand with the purity of more than or equal to 99.99 percent has important economic benefit and practical significance.
Disclosure of Invention
The invention aims to overcome the technical defects and provides a method for preparing 4N high-purity quartz sand by using pegmatite quartz as a raw material, the method can obviously reduce the content of impurity elements in pegmatite quartz to obtain the quartz sand with high purity, the consumption of medicinal agents in the preparation process is low, the process flow is simple, and the technical problems of complex preparation process and low purity of the high-purity quartz sand in the prior art are solved.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the invention provides a method for preparing 4N high-purity quartz sand by taking pegmatite quartz as a raw material, which comprises the following steps:
s1, crushing, grinding and screening pegmatite raw quartz ore to obtain pegmatite raw quartz powder;
s2, after the pegmatite quartz powder is mixed into ore pulp, adjusting the pH value of the ore pulp to 2-3, adding an anionic collector into the ore pulp, stirring, adding a cationic collector, performing flotation treatment, removing impurities to obtain pegmatite quartz concentrate, and cleaning the pegmatite quartz concentrate to be neutral;
s3, roasting the pegmatite quartz concentrate for 3-7 hours at 850-1000 ℃, performing water quenching on the pegmatite quartz concentrate after roasting is finished, removing impurities, and cleaning the pegmatite quartz concentrate after water quenching;
and S4, mixing the roasted pegmatite quartz concentrate subjected to water quenching with a leaching solution, carrying out hot-pressing leaching treatment, wherein the hot-pressing leaching temperature is 220-250 ℃, the hot-pressing leaching time is 4-8 h, the leaching solution is a mixed solution of a sulfuric acid solution and a hydrofluoric acid solution, and after the hot-pressing leaching is finished, washing a hot-pressing leaching product to be neutral, filtering and drying to obtain the 4N high-purity quartz sand.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the method for preparing the high-purity quartz sand by using the pegmatite quartz as the raw material, pegmatite quartz pulp is subjected to flotation through an anion collecting agent and a cation collecting agent under an acidic condition, the anion collecting agent, feldspar and mica are subjected to physical and chemical adsorption, the cation collecting agent, the feldspar and mica are subjected to association and hydrogen bond adsorption, the anion collecting agent and the cation collecting agent form synergistic action, the adsorption of the anion collecting agent and the cation collecting agent on the surfaces of the feldspar and mica is increased, the pulp flotation is promoted, and therefore the separation of gangue minerals and quartz is achieved; then, roasting-water quenching treatment is carried out, in the roasting process of 850-1000 ℃, quartz particles, impurity mineral inclusion bodies, gas-liquid inclusion bodies and the like have different thermal expansion coefficients and receive different expansion acting forces, meanwhile, through the water quenching treatment, the quartz particles are subjected to various actions of cold shrinkage force, internal thermal expansion force and the like, so that cracks are generated on the surfaces of the quartz particles, crystal boundaries, the gas-liquid inclusion bodies and the mineral inclusion bodies, minerals in the impurity mineral inclusion bodies are exposed, meanwhile, trace lattice impurities and the gas-liquid inclusion bodies which are difficult to remove are removed, the contact surface area of subsequent leaching is increased due to the existence of a large number of cracks, and finally, hot-pressing leaching is carried out through sulfuric acid solution and hydrofluoric acid solution at 220-250 ℃, so that Si-O bonds can be better destroyed, and silicate minerals such as mica, feldspar and the like in quartz sand are dissolved and removed; the preparation method has simple process flow, and the prepared 4N quartz sand has higher purity;
2. the method for preparing high-purity quartz sand by taking pegmatite quartz as a raw material provided by the invention uses low SiO 2 Preparing SiO from pegmatite-containing quartz serving as raw material 2 The 4N high-purity quartz sand with the content of more than or equal to 99.99wt% has lower content of impurity elements, can meet the requirement of the industry on the high-purity quartz sand, and also improves the resource utilization rate of pegmatite quartz by taking the pegmatite quartz as a raw material, increases the added value of the pegmatite quartz, and has higher social, economic and environmental benefits;
3. according to the method for preparing the high-purity quartz sand by using pegmatite quartz as the raw material, the sulfuric acid solution and the hydrofluoric acid solution are used as the leaching solutions, impurity elements can be efficiently leached in the hot-pressing leaching process, the medicament consumption is low, and compared with the traditional normal-temperature leaching process, the leaching agent consumption and the leaching time are greatly reduced.
Drawings
FIG. 1 is a flow chart of the process for preparing 4N high-purity quartz sand from pegmatite quartz according to the invention;
FIG. 2 is a micrograph of pegmatite raw ore, FIG. 2 (a) is a view showing quartz (Q), FIG. 2 (b) is a view showing orthoclase (O) and fluid inclusion (M), FIG. 2 (c) is a view showing fluid inclusion (M), and FIG. 2 (D) is a view showing muscovite (D), wherein Q represents quartz, O represents orthoclase, D represents muscovite, and M represents fluid inclusion;
fig. 3 is an XRD pattern of pegmatite quartz raw ore.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
FIG. 1 is a process flow chart of the invention for preparing 4N high-purity quartz sand from pegmatite quartz. As shown in fig. 1, an embodiment of the present invention provides a method for preparing 4N high-purity quartz sand from pegmatite quartz, which comprises the following steps:
(1) Crushing, grinding and screening pegmatite raw quartz to obtain pegmatite quartz powder;
(2) After pegmatite quartz powder is mixed into ore pulp, adjusting the pH value of the ore pulp to 2-3, adding an anionic collector into the ore pulp, stirring, adding a cationic collector, performing flotation treatment, removing impurities to obtain pegmatite quartz concentrate, and cleaning the pegmatite quartz concentrate to be neutral;
(3) Roasting pegmatite quartz concentrate for 3-7 h at 850-1000 ℃, performing water quenching on the pegmatite quartz concentrate after roasting is finished, removing impurities, and cleaning the pegmatite quartz concentrate after water quenching;
(4) Mixing the pegmatite quartz concentrate subjected to roasting and water quenching with a leaching solution, carrying out hot-pressing leaching treatment, wherein the hot-pressing leaching temperature is 220-250 ℃, the hot-pressing leaching time is 4-8 h, the leaching solution is a mixed solution of a sulfuric acid solution and a hydrofluoric acid solution, and after the hot-pressing leaching is finished, washing a hot-pressing leaching product to be neutral, filtering and drying to obtain the 4N high-purity quartz sand.
In the embodiment of the invention, in the step (1), pegmatite quartz raw ore is crushed, ground and sieved to prepare pegmatite quartz powder with the grain size of 50-140 meshes.
In the embodiment of the invention, in the step (2), the content of pegmatite quartz powder in the ore pulp is 10-30 wt%.
In the embodiment of the invention, in the step (2), the pH value of the ore pulp is adjusted to 2-3 by using a sulfuric acid solution with the mass fraction of 10%.
In order to achieve better flotation effect, the anion collector can better perform chemical adsorption and physical adsorption with feldspar and mica, the cation collector can perform association and hydrogen bond adsorption with the feldspar and mica, and the anion collector can have better synergistic effect.
In order to better remove the feldspar and mica minerals with high impurity content, in some preferred embodiments of the invention, in the step (2), the adding amount of the anionic collector is 300-500g.t -1 The adding amount of the cation collecting agent is 600-800g.t -1 Namely, 300-500 g of anion collecting agent is added into each ton of ore pulp, and 600-800 g of cation collecting agent is added into each ton of ore pulp.
In order to further improve the flotation effect on the gangue minerals and save the cost, more preferably, in the step (2), the mass ratio of the anionic collector to the cationic collector is 1:1.5 to 2.
In the embodiment of the invention, in the step (2), after the flotation treatment, the pegmatite quartz concentrate is washed to be neutral by using ultrapure water, and then filtered and vacuum-dried to obtain the pegmatite quartz concentrate after flotation. The vacuum drying temperature and time can be determined by those skilled in the art according to practical conditions, as long as sufficient drying of pegmatite quartz concentrate can be ensured, and the invention is not further limited to this.
In the embodiment of the invention, in the step (3), after the water quenching treatment, the pegmatite quartz concentrate is washed by ultrapure water, and after filtration and vacuum drying, the pegmatite quartz concentrate after the roasting water quenching treatment is obtained. The vacuum drying temperature and time can be determined by those skilled in the art according to practical conditions, as long as sufficient drying of pegmatite quartz concentrate can be ensured, and the invention is not further limited to this.
In order to fully dissolve silicate minerals such as mica and feldspar in quartz, in some preferred embodiments of the invention, in the step (4), the solid-to-liquid ratio of pegmatite quartz concentrate to the leaching solution is 3-6: 1, namely, 1mL of leaching solution is added into every 3 to 6 g of pegmatite quartz concentrate.
In order to achieve better leaching effectIf the gangue minerals and inclusions in the quartz are sufficiently dissolved and removed, in some preferred embodiments of the present invention, the concentration of the sulfuric acid solution in the leachate is 0.3 to 0.7mol.L in step (4) -1 The concentration of the hydrofluoric acid solution is 0.3-0.5mol.L -1 。
In the example of the present invention, in the step (4), siO in 4N high purity silica sand 2 The content is more than or equal to 99.99wt%.
In order to further illustrate the present invention, the following examples are given to further illustrate the present invention. The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified; materials, reagents and the like used in examples of the present invention were commercially available unless otherwise specified.
Example 1:
the embodiment 1 of the invention provides a method for preparing 4N high-purity quartz sand by using pegmatite quartz of Mongolia palustris as a raw material, which comprises the following steps:
(1) Crushing, grinding and screening: crushing pegmatite quartz raw ore by using a jaw crusher, grinding the pegmatite quartz raw ore by using a ball mill, and finally screening the material to 50-140 meshes by using a vibrating screen to obtain pegmatite quartz powder;
(2) Flotation treatment: adding ultrapure water to pegmatite quartz powder, mixing to 10wt%, adding 10wt% of water, and 2 SO 4 the pH of the pulp is adjusted to 2 by the solution, and 300g.t is added -1 Sodium dodecyl sulfate, stirring for 5min, adding 600g.t -1 Performing flotation on laurylamine, starting an inflation valve, stirring for 30s, scraping bubbles until no foam is generated, removing silicate gangue minerals such as feldspar, mica and the like in the pegmatite quartz powder to obtain pegmatite quartz concentrate, and washing, filtering and vacuum-drying the pegmatite quartz concentrate by using ultrapure water;
(3) Roasting and water quenching: placing the flotated pegmatite quartz concentrate into a crucible, roasting the crucible in a muffle furnace at the temperature of 900 ℃ for 7 hours, immediately taking out the pegmatite quartz concentrate after roasting, pouring the pegmatite quartz concentrate into ultrapure water for water quenching treatment, and then washing, filtering and vacuum-drying the pegmatite quartz concentrate by using the ultrapure water;
(4) Hot-pressing leaching: adding the pegmatite quartz concentrate subjected to roasting and water quenching treatment into a hydrothermal reaction kettle (the lining of the hydrothermal reaction kettle is filled with polytetrafluoroethylene) filled with a leaching solution for hot-pressing leaching treatment, wherein the solid-to-liquid ratio of pegmatite quartz concentrate to the leaching solution is 3:1, the concentration of the leaching solution is 0.3mol.L -1 Sulfuric acid solution and concentration of 0.3mol.L -1 A mixed solution of the hydrofluoric acid solution of (a); and (3) carrying out hot-pressing leaching at 250 ℃ for 6h, washing the hot-pressing leaching product to be neutral by using ultrapure water after the hot-pressing leaching is finished, filtering and drying in vacuum to obtain the 4N high-purity quartz sand.
The obtained product is analyzed and tested by ICP-MS, and SiO in quartz sand 2 The contents and the contents of each impurity element are shown in Table 1.
Example 2:
embodiment 2 of the invention provides a method for preparing 4N high-purity quartz sand from invigorated pegmatite quartz, which comprises the following steps:
(1) Crushing, grinding and screening: crushing pegmatite quartz raw ore by using a jaw crusher, grinding the pegmatite quartz raw ore by using a ball mill, and finally screening the material to 50-140 meshes by using a vibrating screen to obtain pegmatite quartz powder;
(2) Flotation treatment: adding ultrapure water into pegmatite quartz powder, mixing to 20wt%, adding 10wt% 2 SO 4 The pH of the pulp is adjusted to 2.5 by the solution and 300g.t is added -1 Sodium dodecyl sulfate, stirring for 5min, adding 600g.t -1 Performing flotation on laurylamine, starting an inflation valve, stirring for 30s, scraping bubbles until no foam is generated, removing silicate gangue minerals such as feldspar, mica and the like in the pegmatite quartz powder to obtain pegmatite quartz concentrate, and washing, filtering and vacuum-drying the pegmatite quartz concentrate by using ultrapure water;
(3) Roasting and water quenching: placing the flotated pegmatite quartz concentrate into a crucible, roasting the crucible in a muffle furnace at the temperature of 1000 ℃ for 6 hours, immediately taking out the pegmatite quartz concentrate after roasting, pouring the pegmatite quartz concentrate into ultrapure water for water quenching treatment, and then washing, filtering and vacuum-drying the pegmatite quartz concentrate by using the ultrapure water;
(4) Hot-pressing leaching: adding the pegmatite quartz concentrate subjected to roasting and water quenching treatment into a hydrothermal reaction kettle (the lining of the hydrothermal reaction kettle is filled with polytetrafluoroethylene) filled with the leachate for hot-pressing leaching treatment, wherein the solid-to-liquid ratio of the pegmatite quartz concentrate to the leachate is 5:1, the concentration of the leaching solution is 0.5mol.L -1 The concentration of the sulfuric acid solution is 0.4mol.L -1 A mixed solution of the hydrofluoric acid solution of (a); and (3) carrying out hot-pressing leaching at the temperature of 240 ℃ for 6h, washing the hot-pressing leaching product to be neutral by using ultrapure water after the hot-pressing leaching is finished, filtering and drying in vacuum to obtain the 4N high-purity quartz sand.
The obtained product is analyzed and tested by ICP-MS, and SiO in quartz sand 2 The contents and the contents of each impurity element are shown in Table 1.
Example 3:
embodiment 3 of the present invention provides a method for preparing 4N high purity quartz sand from pegmatite quartz of inner mongolia somewhere as a raw material, comprising the steps of:
(1) Crushing, grinding and screening: crushing pegmatite quartz raw ore by using a jaw crusher, grinding the pegmatite quartz raw ore by using a ball mill, and finally screening the material to 50-140 meshes by using a vibrating screen to obtain pegmatite quartz powder;
(2) Flotation treatment: adding ultrapure water to pegmatite quartz powder, mixing to 25wt%, adding 10wt% 2 SO 4 The pH of the pulp is adjusted to 3 by the solution, 400g.t is added -1 Sodium dodecyl sulfate, stirring for 5min, adding 700g.t -1 Performing flotation on laurylamine, starting an inflation valve, stirring for 30s, scraping bubbles until no foam is generated, removing silicate gangue minerals such as feldspar, mica and the like in the pegmatite quartz powder to obtain pegmatite quartz concentrate, and washing, filtering and vacuum-drying the pegmatite quartz concentrate by using ultrapure water;
(3) Roasting and water quenching: placing the flotated pegmatite quartz concentrate into a crucible, roasting the crucible in a muffle furnace at the temperature of 1000 ℃ for 5 hours, immediately taking out the pegmatite quartz concentrate after roasting, pouring the pegmatite quartz concentrate into ultrapure water for water quenching treatment, and then washing, filtering and vacuum-drying the pegmatite quartz concentrate by using the ultrapure water;
(4) Hot-pressing leaching: adding the pegmatite quartz concentrate subjected to roasting and water quenching treatment into a hydrothermal reaction kettle (the lining of the hydrothermal reaction kettle is filled with polytetrafluoroethylene) filled with the leachate for hot-pressing leaching treatment, wherein the solid-to-liquid ratio of pegmatite quartz concentrate to the leachate is 6:1, the concentration of the leaching solution is 0.5mol.L -1 And the concentration of the sulfuric acid solution is 0.5mol.L -1 The hydrofluoric acid solution of (a); and (3) carrying out hot-pressing leaching at 250 ℃ for 6h, washing the hot-pressing leaching product to be neutral by using ultrapure water after the hot-pressing leaching is finished, filtering and drying in vacuum to obtain the 4N high-purity quartz sand.
The obtained product is analyzed and tested by ICP-MS, and SiO in quartz sand 2 The contents and the contents of each impurity element are shown in Table 1.
Example 4:
embodiment 4 of the present invention provides a method for preparing 4N high purity quartz sand from pegmatite quartz of inner mongolia somewhere as a raw material, comprising the steps of:
(1) Crushing, grinding and screening: crushing pegmatite quartz raw ore by using a jaw crusher, grinding the pegmatite quartz raw ore by using a ball mill, and finally screening the material to 50-140 meshes by using a vibrating screen to obtain pegmatite quartz powder;
(2) Flotation treatment: adding ultrapure water into pegmatite quartz powder, mixing to 30wt%, adding 10wt% 2 SO 4 The pH of the pulp is adjusted to 3 by the solution, 500g.t is added -1 Sodium dodecyl sulfate, stirring for 5min, and adding 800g.t -1 Performing flotation on laurylamine, starting an inflation valve, stirring for 30s, scraping bubbles until no foam is generated, removing silicate gangue minerals such as feldspar, mica and the like in the pegmatite quartz powder to obtain pegmatite quartz concentrate, and washing, filtering and vacuum-drying the pegmatite quartz concentrate by using ultrapure water;
(3) Roasting and water quenching: placing the flotated pegmatite quartz concentrate into a crucible, roasting the crucible in a muffle furnace at the temperature of 1100 ℃ for 7 hours, immediately taking out the pegmatite quartz concentrate after roasting, pouring the pegmatite quartz concentrate into ultrapure water for water quenching treatment, and then washing, filtering and vacuum-drying the pegmatite quartz concentrate by using the ultrapure water;
(4) Hot-pressing leaching: adding the pegmatite quartz concentrate subjected to roasting and water quenching treatment into a hydrothermal reaction kettle (the lining of the hydrothermal reaction kettle is filled with polytetrafluoroethylene) filled with the leachate for hot-pressing leaching treatment, wherein the solid-to-liquid ratio of pegmatite quartz concentrate to the leachate is 6:1, the concentration of the leaching solution is 0.7mol.L -1 Sulfuric acid solution of (2) and a concentration of 0.5mol.L -1 A mixed solution of the hydrofluoric acid solution of (a); and (3) carrying out hot-pressing leaching at 250 ℃ for 8h, washing the hot-pressing leaching product to be neutral by using ultrapure water after the hot-pressing leaching is finished, filtering and drying in vacuum to obtain the 4N high-purity quartz sand.
The obtained product is analyzed and tested by ICP-MS, and SiO in quartz sand 2 The contents and the contents of each impurity element are shown in Table 1.
Fig. 2 and 3 are a micrograph and an XRD pattern, respectively, of pegmatite quartz raw ore used in examples 1 to 4 of the present invention. Fig. 2 (a) is a view of quartz (Q), fig. 2 (b) is a view of orthoclase (O) and fluid inclusion (M), fig. 2 (c) is a view of fluid inclusion (M), and fig. 2 (D) is a view of muscovite (D), where Q represents quartz, O represents orthoclase, D represents muscovite, and M represents fluid inclusion, and as can be seen from fig. 2, the pegmatite raw ore contains a large amount of impurities, and the main gangue minerals in the pegmatite raw ore are orthoclase, muscovite, and the like, and further impurities such as fluid inclusion are present. Fig. 3 is an XRD pattern of pegmatite quartz raw ore, and it can be seen from fig. 3 that pegmatite quartz mainly contains quartz and other small amounts of other impurities.
TABLE 1 SiO of pegmatite raw ores and products of the examples 2 Content and content of each impurity element
As can be seen from Table 1, siO of 4N high purity silica sand prepared in examples 1 to 4 of the present invention 2 The content can at least reach more than 99.99wt%, and impurity elements such as Al, fe, na, K and the likeThe content of the quartz sand is far lower than that of pegmatite raw ore, the prepared high-purity quartz sand can meet the requirement of the industry on the high-purity quartz sand, the consumption of the medicament in the preparation process is less, and the process flow is simple.
The above-described embodiments of the present invention should not be construed as limiting the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the protection scope of the claims of the present invention.
Claims (6)
1. The method for preparing 4N high-purity quartz sand by taking pegmatite quartz as a raw material is characterized by comprising the following steps of:
s1, crushing, grinding and screening pegmatite raw ore to obtain pegmatite raw ore powder;
s2, after the pegmatite quartz powder is mixed into ore pulp, adjusting the pH value of the ore pulp to 2-3, adding an anionic collector into the ore pulp, stirring, adding a cationic collector, performing flotation treatment, removing impurities to obtain pegmatite quartz concentrate, and cleaning the pegmatite quartz concentrate to be neutral;
s3, roasting the pegmatite quartz concentrate for 3-7 hours at 850-1000 ℃, performing water quenching on the pegmatite quartz concentrate after roasting is finished, removing impurities, and cleaning the pegmatite quartz concentrate after water quenching;
s4, mixing the pegmatite quartz concentrate subjected to roasting and water quenching with a leaching solution, carrying out hot-pressing leaching treatment, wherein the hot-pressing leaching temperature is 220-250 ℃, the hot-pressing leaching time is 4-8 h, the leaching solution is a mixed solution of a sulfuric acid solution and a hydrofluoric acid solution, after the hot-pressing leaching is finished, washing a hot-pressing leaching product to be neutral, filtering and drying to obtain 4N high-purity quartz sand, the particle size of pegmatite quartz powder is 50-140 meshes, the content of pegmatite quartz powder in the ore pulp is 10-30 wt%, the anionic collector is sodium dodecyl sulfate, the cationic collector is dodecylamine, and the mass ratio of the anionic collector to the cationic collector is 1:1.5 to 2.
2. The method for preparing 4N high-purity quartz sand using pegmatite quartz as a raw material according to claim 1, wherein the pH of the ore pulp is adjusted to 2 to 3 by using a sulfuric acid solution with a mass fraction of 10%.
3. The method for preparing 4N high-purity quartz sand from pegmatite quartz as claimed in claim 1, wherein the addition amount of the anionic collector is 300 to 500 g.t-1, and the addition amount of the cationic collector is 600 to ℃
800 g.t-1。
4. The method for preparing 4N high-purity quartz sand from pegmatite quartz as claimed in claim 1, wherein the solid-to-liquid ratio of pegmatite quartz concentrate to leaching solution is 3-6: 1, wherein the unit of solid is g, the unit of liquid is mL, namely 1mL of leaching solution is added into every 3 to 6 grams of pegmatite quartz concentrate.
5. The method for preparing 4N high purity quartz sand using pegmatite quartz as a raw material according to claim 1, wherein the concentration of the sulfuric acid solution in the leachate is 0.3 to 0.7mol.L-1, and the concentration of the hydrofluoric acid solution is 0.3 to 0.5 mol.L-1.
6. The method for preparing 4N high-purity quartz sand from pegmatite quartz as claimed in claim 1, wherein SiO in the 4N high-purity quartz sand is 2 The content is more than or equal to 99.99wt%.
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| CN114014540B (en) * | 2021-12-08 | 2022-07-29 | 连云港太平洋半导体材料有限公司 | Preparation process of opal quartz glass |
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| CN115140741B (en) * | 2022-06-30 | 2023-07-21 | 中鸿控股集团有限公司 | Preparation of 4N and above 4N SiO using granite pegmatite as raw material 2 Method for producing quartz sand |
| CN115849393A (en) * | 2022-08-01 | 2023-03-28 | 西南科技大学 | High-purity quartz and preparation method thereof |
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